CN114749210B - Preparation method and application of catalyst of room temperature end-capped 107 glue - Google Patents

Preparation method and application of catalyst of room temperature end-capped 107 glue Download PDF

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CN114749210B
CN114749210B CN202210430300.8A CN202210430300A CN114749210B CN 114749210 B CN114749210 B CN 114749210B CN 202210430300 A CN202210430300 A CN 202210430300A CN 114749210 B CN114749210 B CN 114749210B
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reaction
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CN114749210A (en
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张建
刘国栋
陈怀良
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Shandong Copolymer Silicone Technology Research Institute Co ltd
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Jining University
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
    • B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
    • B01J31/04—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing carboxylic acids or their salts
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
    • B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
    • B01J31/0215—Sulfur-containing compounds
    • B01J31/0225—Sulfur-containing compounds comprising sulfonic acid groups or the corresponding salts
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
    • B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
    • B01J31/0234—Nitrogen-, phosphorus-, arsenic- or antimony-containing compounds
    • B01J31/0235—Nitrogen containing compounds
    • B01J31/0237—Amines
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
    • B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
    • B01J31/12—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing organo-metallic compounds or metal hydrides
    • B01J31/14—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing organo-metallic compounds or metal hydrides of aluminium or boron
    • B01J31/146—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing organo-metallic compounds or metal hydrides of aluminium or boron of boron
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04—Polysiloxanes
    • C08G77/38—Polysiloxanes modified by chemical after-treatment
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
    • C08L83/04—Polysiloxanes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24—Acids; Salts thereof
    • C08K3/26—Carbonates; Bicarbonates
    • C08K2003/265—Calcium, strontium or barium carbonate
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/584—Recycling of catalysts

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  • General Chemical & Material Sciences (AREA)
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Abstract

The invention discloses a preparation method and application of a catalyst of room temperature end-capped 107 glue, and belongs to the technical field of organic silicon materials. The technical proposal is as follows: the preparation method of the catalyst of the room temperature end-capped 107 glue is characterized by comprising the following steps: 1) Adding phosphoric acid into water, heating, and adding organic alcohol under stirring for reaction; 2) Preparing a saturated aqueous solution of an active organic matter, and dropwise adding the saturated aqueous solution into the reaction solution in the step 1) to continue the reaction; 3) After the reaction is finished, the temperature is raised, the vacuum is reduced, and the solid product catalyst is obtained. The room-temperature-terminated 107 catalyst prepared by the invention has the advantages of simple preparation process, readily available raw materials, environmental friendliness, suitability for large-scale industrial production and wide application prospect.

Description

Preparation method and application of catalyst of room temperature end-capped 107 glue
Technical Field
The invention relates to the technical field of organic silicon materials, in particular to a preparation method of a catalyst of room-temperature end-capped 107 glue.
Background
The dealcoholized room temperature vulcanized silicone rubber is environment-friendly due to the release of small molecular methanol or ethanol, has no corrosion to metal and no pungent smell, and is widely applied to the industries of electronics, buildings, automobiles and the like. The dealcoholized room temperature vulcanized silicone rubber is prepared by taking alpha, omega-dihydroxyl polydimethylsiloxane (also called 107 glue) as a base glue, adding a plasticizer, a cross-linking agent, a coupling agent, a filler and a catalyst for adjustment, and then stirring in vacuum. Wherein the catalyst is typically a titanate-based catalyst. However, titanate is easy to cause viscosity peak of sizing materials in the preparation process, and instrument damage and production damage can be caused when the viscosity peak is severe. The problem of viscosity peaks can be effectively solved after the alkoxy end capping of 107 silicone rubber, so the preparation process of the alkoxy end capping 107 becomes a very concerned research subject for researchers.
The alkoxy end-capping 107 mainly comprises direct end-capping of a catalyst, hydrolytic polycondensation of a monomer, and the like. For example, the invention patent (CN 104479132B) provides an alkoxy end-capped 107 glue and a preparation method thereof, wherein dimethyl dichlorosilane and 107 glue are reacted to obtain dichloro polydimethylsiloxane, after hydrogen chloride is removed, alkoxysilane and dichloro polydimethylsiloxane are reacted to obtain the alkoxy end-capped 107, a byproduct Hcl needs to be removed, and a post-treatment step is complicated. The invention patent (CN 110878142A) provides a synthesis method of alkoxy end-capped polysiloxane and the alkoxy end-capped polysiloxane, which are prepared by adding platinum catalyst into vinyl silicone oil and alkoxy hydrosilane serving as raw materials and performing hydrosilylation reaction, wherein noble metal is needed in the preparation process, and the preparation cost is high. The invention patent (CN 104231275B) provides a preparation method of alkoxy-terminated silicone oil, which comprises the steps of adding a catalyst into hydroxyl-terminated polydimethylsiloxane and alkoxy silane, heating, reacting, neutralizing, filtering, distilling under reduced pressure to obtain the alkoxy silicone oil, and after the reaction is finished, the alkoxy silicone oil is also required to be neutralized and filtered, and the process is complex and the operation is complicated. In addition, the end-capping process in the prior art needs to wait until the end-capping 107 is cooled to room temperature before being used as the base rubber of the dealcoholized room temperature vulcanized silicone rubber, so that the process flow is prolonged, and the energy consumption is increased. Thus, there is an urgent need for catalysts that can achieve end capping 107 at room temperature.
Disclosure of Invention
The invention aims to solve the technical problems that: overcomes the defects of the prior art and provides a preparation method of a catalyst of room temperature end-capped 107 glue to solve the problems.
The technical scheme of the invention is as follows:
in a first aspect, a method for preparing a catalyst for room temperature end-capped 107 glue is provided, comprising the steps of:
1) Adding phosphoric acid into water, heating, and adding organic alcohol under stirring for reaction;
2) Preparing a saturated aqueous solution of an active organic matter, and dropwise adding the saturated aqueous solution into the reaction solution in the step 1) to continue the reaction;
3) After the reaction is finished, the temperature is raised, the vacuum is reduced, and the solid product catalyst is obtained.
Preferably, the organic alcohol in step 1) is one or more of propanol, butanol, pentanol, hexanol, heptanol, octanol, ethylene glycol, propylene glycol, butylene glycol, pentylene glycol, hexylene glycol, glycerol and pentaerythritol.
Preferably, the active organic matter in step 2) is one of aminobenzoic acid, aminobenzenesulfonic acid, aminophenylboronic acid and aminosalicylic acid, preferably aminobenzoic acid.
Preferably, the reaction temperature in step 1) is from 40 ℃ to 160 ℃; the reaction time is 0.5h-4h.
Preferably, the reaction temperature in step 1) is from 60 ℃ to 140 ℃; the reaction time is 1h-3h.
Preferably, the reaction time in step 2) is from 0.5h to 4h, preferably from 1h to 3h.
Preferably, the vacuum conditions in step 3) are-0.05 MPa-0.1 MPa, preferably-0.06 MPa-0.09 MPa.
Preferably, the phosphoric acid: active organic matter: organic alcohol: water (molar ratio) =1: (1-2): (0.5-2): (10-50).
In another aspect, the use of a catalyst in the preparation of dealcoholized vulcanized silicone rubber is disclosed.
The reaction mechanism is as follows: the acidity of phosphoric acid is reduced, and the corresponding ester is produced by the reaction of alcohols with phosphoric acid. The structural stability of the product is enhanced, the acidity of the product is further reduced, and the gelation in the end capping process is avoided. And then the phosphoric acid reacts with amino in the active organic matters to graft the active organic matters onto the phosphoric acid, and active groups (carboxyl groups, sulfonic groups and boric groups) in the organic matters are reserved. The product catalyst of the invention uses the acid group in the structure to react with the alkoxy silane end capping agent to remove methanol or ethanol and coordinate with silicon atoms of silane. The amino group in the product structure will react with the hydroxyl end group of 107 and bond it to the silicon atom of the silane, completing the capping process. In addition, the benzene ring structure in the active organic matter promotes the compatibility between the catalyst and 107 glue, enhances the activity between reactants, and avoids the defects of low catalytic activity and uneven dispersion of other types of catalysts caused by phase incompatibility.
Compared with the prior art, the invention has the following beneficial effects:
1. the catalyst capable of blocking 107 glue at room temperature, which is prepared by the invention, has the advantages of simple preparation process, easily available raw materials, environmental friendliness, suitability for large-scale industrial production and wide application prospect;
2. the catalyst capable of blocking 107 glue at room temperature, which is prepared by the invention, has excellent blocking performance for 107 glue, can realize room temperature blocking effect, and solves the technical problems of high blocking cost, high temperature requirement and the like;
3. the alkoxy end-capped 107 rubber prepared by the catalyst of the invention is used as a base rubber of dealcoholized silicone rubber, and the storage period can be prolonged to 18 months.
Drawings
FIG. 1 is an infrared spectrum of the product catalyst prepared in example 1 of the present invention.
FIG. 2 is an infrared spectrum of the modified 107 glue prepared in example 6 of the present invention.
Detailed Description
Example 1
The room temperature end-capped 107 catalyst was prepared in this example, and the specific steps were as follows:
1) Weighing 5g of phosphoric acid, adding the phosphoric acid into 20g of pure water, heating to 85 ℃, dropwise adding 6.6g of n-hexanol, and reacting for 2 hours;
2) A saturated aqueous solution of para-aminobenzoic acid (content of para-aminobenzoic acid 8.5 g) was added dropwise to the above solution and the reaction was continued for 2 hours;
3) After the reaction is finished, the temperature is raised to 120 ℃, the vacuum is pumped to-0.098 MPa, unreacted alcohol and water are removed, and a solid product catalyst is obtained, and an infrared spectrum of the catalyst is shown in figure 1.
Example 2
As described in example 1, example 2 was different from example 1 in that a saturated aqueous solution of aminosalicylic acid (aminosalicylic acid content: 7.6 g) was added in step 2), and the other reaction conditions were the same.
Example 3
As described in example 1, example 3 was different from example 1 in that a saturated aqueous solution of aminophenylboronic acid (the aminophenylboronic acid content was 6 g) was added in step 2), and the other reaction conditions were the same.
Example 4
Example 4 differs from example 1 in that 2g of 1, 3-propanediol was added in step 1) as described in example 1, all other reaction conditions being identical.
Example 5
Example 5 differs from example 1 in that the reaction temperature in step 1) is 160℃and the other reaction conditions are the same as in example 1.
Examples 6 to 10
The method for preparing the modified 107 glue by using the catalysis prepared in examples 1 to 5 is as follows:
300g of 20000 mPa.s terminal hydroxyl polydimethylsiloxane (107 glue) and 2.0g of vinyltrimethoxysilane were weighed, 0.1g of the catalyst prepared in examples 1-5 was added respectively, and the mixture was stirred at room temperature for one hour to prepare a modified 107 glue, and the modified 107 glue prepared in example 6 was subjected to infrared spectroscopic measurement, and the result is shown in FIG. 2.
Comparative example 1
300g of 20000 mPa.s terminal hydroxyl polydimethylsiloxane (107 glue) and 2.0g of vinyltrimethoxysilane were weighed and stirred at normal temperature for one hour to prepare modified 107 glue.
Examples 6-10 modified 107 gums were prepared and comparative example 1 was tested for the presence of viscosity peaks by adding tetraisopropyl titanate. Under rapid stirring, 1mL of tetraisopropyl titanate was added to 10g of modified 107 gel, and the presence of a viscosity peak was judged by observing whether or not the rapid increase in the viscosity of modified 107 gel occurred. The test results are shown in table 1,
TABLE 1
Examples viscosity/mPa.s Peak viscosity
Example 6 18000 Without any means for
Example 7 17500 Without any means for
Example 8 18600 Without any means for
Example 9 17000 Without any means for
Example 10 17700 Without any means for
Comparative example 1 20000 Peak
Example 11
1000g of modified 107 glue with the viscosity of 18000 mPa.s prepared in application example 6, 800g of active nano calcium carbonate and 50g of simethicone are added into a dispersion glue making machine to obtain premix. 30g of methyltrimethoxysilane, 5g of KH-560, 10g of titanate chelate and 0.5g of organotin catalyst are added, and the mixture is vacuumized and stirred for 30 minutes to obtain the dealcoholized silicone rubber.
Comparative example 2
Comparative example 2 was different from example 11 in that 107 gums having a viscosity of 20000 mPas prepared in comparative example 1 were used, and the remaining reaction conditions were the same.
The surface dry tack-free performance of the silicone rubber after conventional (room temperature vulcanization) and aging (aging at 90 ℃ for 3 days) is tested, and the tack-free time of the single-component silicone rubber is qualified within 3 hours and within 24 hours under standard conditions (temperature (23+/-2) ℃ and relative humidity (50+/-5)) according to the GB16776-2005 test. The dealcoholized silicone rubber is stored in a rubber bottle in a sealing way, and then is aged for 3 days at 90 ℃ which is equivalent to 18 months at room temperature. The properties of the silicone rubbers prepared in example 11 and comparative example 2 are shown in table 2:
TABLE 2
Figure BDA0003610031350000061
As can be seen from FIG. 1, 2929cm -1 Is a characteristic peak of methylene, 1700cm -1 Characteristic absorption peak of c=o, 1277cm -1 Is the characteristic absorption peak of phosphate, 766cm -1 The formation of phosphate is further illustrated by the characteristic peak of P-O-C. 3132cm -1 Is NH 3 + Characteristic peaks, which indicate that amino acids form a coordination structure with phosphoric acid. 2658cm -1 Is a P-OH stretching vibration peak, 1495cm -1 、1528cm -1 、1604cm -1 The successful preparation of the product catalyst is verified for the characteristic absorption peak of the benzene ring after the benzene ring is substituted by amino and carboxyl.
As can be seen from FIG. 2, 2962cm -1 Characteristic absorption peak of Si-CH3, 1009cm -1 Is a characteristic absorption peak of Si-O-Si, 1412cm -1 Characteristic absorption peak of c=c, 1078cm -1 The characteristic absorption peak of-OCH 3, the hydroxyl peak is basically disappeared, which indicates that the end capping is successful.
As can be seen from Table 1, the viscosity peaks of comparative example 1 still exist, and the viscosity peaks of the thiol-removed silicone rubbers prepared in examples 6 to 10 do not exist, which indicates that the modified 107 rubbers prepared in examples 6 to 10 can be successfully capped under normal temperature conditions.
As can be seen from Table 2, example 11, which uses the modified 107 glue prepared from the catalyst of the present application, and the thiol-modified 107 glue prepared from the modified 107 glue, shows excellent surface drying and viscosity-eliminating properties under conventional conditions and after aging, whereas comparative example 2 only has surface drying and viscosity-eliminating properties under conventional conditions, and does not surface drying and viscosity-eliminating properties after aging, indicating that the catalyst of the present application can prolong the aging properties of the thiol-eliminating silicone rubber, mainly because the catalyst uses the acidic groups in the structure to react with the alkoxysilane capping agent, remove methanol or ethanol, and coordinate with the silicon atoms of the silane. The amino group in the product structure will react with the hydroxyl end group of 107 and bond it to the silicon atom of the silane, completing the capping process. In addition, the benzene ring structure in the active organic matter promotes the compatibility between the catalyst and 107 glue, enhances the activity between reactants, and avoids the defects of low catalytic activity and uneven dispersion of other types of catalysts caused by phase incompatibility.
The room-temperature-terminated 107 catalyst prepared by the invention has the advantages of simple preparation process, readily available raw materials, environmental friendliness, suitability for large-scale industrial production and wide application prospect; the catalyst capable of being blocked at room temperature, which is prepared by the invention, is excellent in blocking performance for 107 glue, can realize the blocking effect at room temperature, and solves the technical problems of high blocking cost, high temperature requirement and the like; the alkoxy end-capped 107 prepared by the catalyst of the invention is used as a base rubber of dealcoholized silicone rubber, and can prolong the storage period to 18 months.
Although the present invention has been described in detail by way of preferred embodiments with reference to the accompanying drawings, the present invention is not limited thereto. Various equivalent modifications and substitutions may be made in the embodiments of the present invention by those skilled in the art without departing from the spirit and scope of the present invention, and it is intended that all such modifications and substitutions be within the scope of the present invention/be within the scope of the present invention as defined by the appended claims. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.

Claims (10)

1. The preparation method of the catalyst of the room temperature end-capped 107 glue is characterized by comprising the following steps:
1) Adding phosphoric acid into water, heating, and adding organic alcohol under stirring for reaction;
2) Preparing a saturated aqueous solution of an active organic matter, and dropwise adding the saturated aqueous solution into the reaction solution in the step 1) to continue the reaction;
3) After the reaction is finished, heating and vacuum removing unreacted alcohol and water to obtain a solid product catalyst;
the active organic matter in the step 2) is one of aminobenzoic acid, aminobenzenesulfonic acid, aminophenylboronic acid and aminosalicylic acid;
the reaction temperature in the step 1) is 40-160 ℃; the reaction time is 0.5h-4h.
2. The method for preparing the catalyst of room temperature end-capped 107 glue of claim 1, wherein: the organic alcohol in the step 1) is one or more of propanol, butanol, amyl alcohol, hexanol, heptanol, octanol, ethylene glycol, propylene glycol, butanediol, pentanediol, hexanediol, glycerol and pentaerythritol.
3. The method for preparing the catalyst of room temperature end-capped 107 glue of claim 1, wherein: the active organic matter in the step 2) is aminobenzoic acid.
4. The method for preparing the catalyst of room temperature end-capped 107 glue of claim 1, wherein: the reaction temperature in the step 1) is 60-140 ℃; the reaction time is 1h-3h.
5. The method for preparing the catalyst of room temperature end-capped 107 glue of claim 1, wherein: the reaction time in the step 2) is 0.5h-4h.
6. The method for preparing the catalyst of room temperature end-capped 107 glue of claim 1, wherein: the reaction time in the step 2) is 1h-3h.
7. The method for preparing the catalyst of room temperature end-capped 107 glue of claim 1, wherein: the vacuum condition in the step 3) is-0.05 MPa to-0.1 MPa.
8. The method for preparing the catalyst of room temperature end-capped 107 glue of claim 1, wherein: the vacuum condition in the step 3) is-0.06 MPa to-0.09 MPa.
9. The method for preparing the catalyst of room temperature end-capped 107 glue of claim 1, wherein: phosphoric acid: active organic matter: organic alcohol: the molar ratio of water is 1: (1-2): (0.5-2): (10-50).
10. The use of a catalyst prepared by the method for preparing a catalyst for room temperature end-capped 107 glue as defined in any one of claims 1-9 for preparing an alkoxy end-capped 107 glue and as a base glue for dealcoholized silicone rubber.
CN202210430300.8A 2022-04-22 2022-04-22 Preparation method and application of catalyst of room temperature end-capped 107 glue Active CN114749210B (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103122063A (en) * 2013-02-05 2013-05-29 中北大学 Preparation method of poly-p-aminobenzoylamonoundecylamine
CN105237783A (en) * 2015-11-21 2016-01-13 唐山三友硅业有限责任公司 Pretreatment method for base rubber of single-component dealcoholized type room temperature vulcanized silicone rubber
CN105367743A (en) * 2015-12-21 2016-03-02 中国科学院山西煤炭化学研究所 Synthetic method of waterborne polyurethane emulsion
CN107715873A (en) * 2017-10-26 2018-02-23 湘潭大学 A kind of preparation method and application using metal-organic framework materials as the carrier loaded La Pt base catalyst being modified
CN110527481A (en) * 2019-09-06 2019-12-03 安徽斯迈特新材料有限公司 A kind of oil-resistant high-temperature silicone sealant and preparation method thereof

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB201613399D0 (en) * 2016-08-03 2016-09-14 Dow Corning Cosmetic composition comprising silicone materials

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103122063A (en) * 2013-02-05 2013-05-29 中北大学 Preparation method of poly-p-aminobenzoylamonoundecylamine
CN105237783A (en) * 2015-11-21 2016-01-13 唐山三友硅业有限责任公司 Pretreatment method for base rubber of single-component dealcoholized type room temperature vulcanized silicone rubber
CN105367743A (en) * 2015-12-21 2016-03-02 中国科学院山西煤炭化学研究所 Synthetic method of waterborne polyurethane emulsion
CN107715873A (en) * 2017-10-26 2018-02-23 湘潭大学 A kind of preparation method and application using metal-organic framework materials as the carrier loaded La Pt base catalyst being modified
CN110527481A (en) * 2019-09-06 2019-12-03 安徽斯迈特新材料有限公司 A kind of oil-resistant high-temperature silicone sealant and preparation method thereof

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